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研究生：	陳雨晶 Chen, Yu-Jing
論文名稱：	用溼式法製備鍶置換氫氧基磷灰石之研究 The study of strontium-substituted hydroxyapatite by wet process
指導教授：	李澤民 Lee, Tzer-Min
學位類別：	碩士 Master
系所名稱：	醫學院 - 口腔醫學研究所 Institute of Oral Medicine
論文出版年：	2012
畢業學年度：	100
語文別：	中文
論文頁數：	91
中文關鍵詞：	鍶置換氫氧基磷灰石、共沉澱法、水熱法、熱穩定性、燒結行為
外文關鍵詞：	strontium-substituted hydroxyapatite, co-precipitation method, hydrothermal method, thermal stability, sintering behavior
相關次數：	點閱：127 下載：3
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傳統處理的鍶置換氫氧基磷灰石(Sr-HA)缺乏均勻性及雜相含量高，在燒結緻密時通常需要高溫處理，但高溫處理會造成晶粒過成長和相分解，導致材料缺乏化學穩定性而降低機械性質。因此本研究使用水熱法合成粉末，製備出純度高、均勻的粉末，在較低溫度下進行燒結處理，避免因高溫處理造成材料機械強度降低。
首先利用共沉澱法(Co-precipitation method)和水熱法(Hydrothermal method)合成不同比例之0, 1, 5, 10 atom% Sr-HA，此為探討不同製備方法對Sr-HA粉末及燒結體的影響。X-ray繞射儀與EDS鑑定粉末的相組成及成份。結果此二種方法製備出來的Sr-HA粉末皆無雜相產生，且(Ca+Sr)/P符合1.67，Sr/(Ca+Sr)的值皆符合理論值。在熱性質分析方面，水熱法合成的Sr-HA粉末具有良好的熱穩定性，鍶含量的添加會使粉末熱穩定性變差。在燒結行為分析中，將乾燥Sr-HA粉末壓成塊材，進行800oC、900oC和1000oC各2小時的燒結處理，探討其燒結行為。以SEM觀察燒結體的表面形態，發現在燒結溫度800oC、900oC只有頸縮現象，在燒結溫度1000oC有明顯的晶粒成長現象，水熱法之Sr-HA燒結體較為緻密，且發現隨著鍶含量增加，緻密化現象愈差，原因是鍶會抑制晶粒的成長。最後利用維氏硬度機量測燒結體的表面硬度，發現水熱法的Sr-HA燒結體硬度較高。上述結果證實不同合成方法會影響粉末的燒結行為，由其以水熱法製備之Sr-HA粉末具有良好的燒結行為，預期未來水熱法製備之Sr-HA粉末在骨填充物材料方面具有很大的發展潛力。

Conventionally processed strontium-substituted hydroxyapatite (Sr-HA) materials are very challenging to sinter; densification has typically required high temperatures but high temperature would result in grain growth and decomposition which induce poor mechanical and chemical stability. In this study, hydrothermal method was used to prepare Sr-HA powders with phase purity and homogeneity. Sr-HA powders as high quality apatite-based bioceramics can be generated at low sintering temperatures.
Co-precipitation and hydrothermal method were used to prepare Sr-HA powders. Sr-HA powders were synthesized at 0, 1, 5, and 10 atom% of strontium contents, respectively. The aim of this study was to investigate the effects of different methods on the properties of Sr-HA powders and sintered bodies. X-ray diffraction and EDS were used to investigate composition of the powders. The results showed that the calculated (Ca+Sr)/P ratio and Sr/(Ca+Sr) ratios were close to the stoichiometric value. No decomposition was identified by X-ray diffraction. In the thermal analysis, powders of hydrothermal synthesis had good thermal stability, and Sr content increased powders were thermally unstable. In the sintering behavior, the dried powder was hydrostatically pressed into disk-shaped compacts and then compacts were sintered at 800oC, 900 oC, and 1000 oC for 2h. The obtained Sr-HA sintered bodies had high density at 1000 oC. Sintered bodies of hydrothermal method were denser and found that as the strontium content increased, the densification was worse due to strontium inhibiting grain growth. A micro-Vickers indentation method was carried out to determine the Vickers hardness and found sintered bodies of hydrothermal method were higher hardness. In conclusion, it was showed that the different methods affect sintering behavior, and Sr-HA powders of hydrothermal method have excellent potential for bone filler applications in the future.

摘要	II
Abstract	III
誌謝	V
目錄	VI
表目錄	IX
圖目錄	X
第一章	緒論	1
1-1生醫材料的分類	1
1-2生醫材料的應用	2
第二章	文獻回顧與理論基礎	4
2-1 氫氧基磷灰石	4
  2-1-1氫氧基磷灰石的基本性質	4
  2-1-2氫氧基磷灰石在室溫下水溶液中之穩定性	4
2-2氫氧基磷灰石的離子置換	4
  2-2-1一般離子的置換種類	4
  2-2-2鍶離子的置換	5
2-3氫氧基磷灰石的高溫相穩定性	6
2-4結晶理論與機制	8
  2-4-1成核理論	8
  2-4-2晶體成長	9
  2-4-3溶質濃度與晶體成核、成長之關係	9
  2-4-4自由能之影響	10
2-5氫氧基磷灰石的合成	11
2-6共沉澱法	12
2-7水熱法	13
  2-7-1水熱法原理	13
  2-7-2水熱法優點	14
2-8固相燒結理論	15
  2-8-1固相燒結模式	15
  2-8-2晶粒成長	15
  2-8-3凝聚體粉末之燒結行為	16
2-9研究目的	16
第三章	材料及方法	18
3-1實驗藥品	18
3-2 實驗步驟及相關參數	18
  3-2-1共沉法	18
  3-2-2水熱法	18
3-3 粉末備製	19
  3-3-1共沉法	19
  3-3-2水熱法	19
3-4 粉末性質分析	20
  3-4-1成分分析	20
  3-4-2 相組成分析	20
  3-4-3微結構分析	21
  3-4-4傅立葉轉換紅外線吸收光譜分析(FT-IR spectrum)	21
  3-4-5 粉末熱分析	22
  3-4-6 粉末BET比表面積分析	22
3-5燒結製程	22
  3-5-1比重量測	23
  3-5-2表面顯微觀察	23
  3-5-3 X光結晶繞射分析	23
  3-5-4表面硬度量測	23
第四章	結果	25
4-1粉末結晶相分析	25
  4-1-1製備方法 I：共沉法	25
  4-1-2製備方法II：水熱法	26
4-2粉末成分分析	27
4-3粉末相鑑定	27
  4-3-1繞射峰繞射角度之變化	27
  4-3-2結晶粒徑(crystallite size)	28
  4-3-3晶格常數a、c和體積、密度	28
4-4粒子形態分析	28
4-5傅立葉轉換紅外線吸收光譜	29
4-6粉末熱性質分析	29
4-7燒結製程分析	30
  4-7-1粉末比表面積分析	30
  4-7-2 Sr-HA燒結體之相對密度	31
  4-7-3 Sr-HA燒結體之表面微觀分析	31
  4-7-4 Sr-HA燒結體之X光結晶繞射分析	31
  4-7-5 Sr-HA燒結體之硬度量測分析	32
第五章	討論	33
第六章	結論	39
參考文獻	41


                                    

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